16 results about "Hafnium tetrachloride" patented technology

This invention relates to the field of hafnium carbide technology and discloses a thermal decomposition preparation process for hafnium carbide precursors. The process includes: dissolving hafnium tetrachloride in anhydrous ethanol, adding propylene oxide dropwise for neutralization and acid removal to obtain a neutral ethanol-hafnium precursor solution; adding ethyl acetoacetate methacrylate and heating for coordination to obtain a hafnium coordination monomer solution; adding acrylonitrile and an initiator and heating for polymerization; when the viscosity of the reaction solution increases, injecting a dimethyl sulfoxide hot solution of melamine as a locking liquid; precipitating, separating, and drying to obtain the hafnium carbide precursor; and after oxidative crosslinking treatment, calcining at high temperature under an inert atmosphere to undergo carbothermic reduction to obtain hafnium carbide powder. This invention achieves molecular-level dispersion of precursor components through liquid-phase coordination and in-situ network locking, effectively reducing the reaction temperature and inhibiting grain agglomeration, thus producing high-purity, ultrafine hafnium carbide powder.

The invention relates to a method for preparing (cyclopentadienyl) tris (dimethylamino) hafnium by using nuclear magnetic control, which comprises the following steps: S1, carrying out heating reflux reaction on hafnium tetrachloride, cyclopentadiene and dimethylamine in the presence of n-butyllithium and n-hexane, and after reacting for a certain time, taking supernate to detect a nuclear magnetic hydrogen spectrum; s2, calculating the ratio a of the integral area of the characteristic peak A to the integral area of the characteristic peak B according to the nuclear magnetic hydrogen spectrum, judging whether a is in a target range or not, if a is in the target range, terminating the reaction, separating a liquid phase, distilling and collecting a crude product; and if a value is greater than the maximum value of the target range, adding cyclopentadiene into the reaction system to continue the reaction, and if a value is less than the minimum value of the target range, continuing the reaction until the ratio of the integral area of the characteristic peak A to the integral area of the characteristic peak B in the nuclear magnetic hydrogen spectrum of the reaction supernatant is within the target range, terminating the reaction, separating the liquid phase, distilling and collecting a crude product. The method can effectively improve the safety of the production process, the raw material conversion rate and the product purity.

The invention provides a method for preparing butyl hafnate from hafnium tetrachloride. The method comprises the following steps: (1) under the protection of inert gas, adding n-butyl alcohol and an organic solvent into a reaction kettle, and then adding hafnium tetrachloride to obtain an initial reaction system; (2) adding a hafnium-based organic metal framework catalyst into the initial reaction system, heating to 40-65 DEG C, controlling the reaction pressure to be 0.1-0.3 MPa, and stirring to react for 3-8 hours to obtain esterification reaction liquid; (3) cooling the esterification reaction liquid to 20-30 DEG C, and separating out solid components in the system by pressure filtration to obtain filtrate; and (4) sequentially carrying out atmospheric distillation, vacuum rectification and precision filtration on the filtrate to obtain the butyl hafnate. By using the hafnium-based catalyst, the reaction efficiency and the product purity of preparing the butyl hafnate from hafnium tetrachloride are improved, and side reaction and equipment corrosion are effectively inhibited. The method is mild in process condition and suitable for industrial large-scale production of butyl hafnate.

The application provides a method for preparing butyl hafnate from hafnium tetrachloride. The method comprises the following steps: (1) adding n-butanol and an organic solvent into a reaction kettle under the protection of inert gas, and then adding hafnium tetrachloride to obtain an initial reaction system; (2) adding a hafnium-based organometallic framework catalyst into the initial reaction system, heating to 40-65 DEG C, controlling the reaction pressure to be 0.1-0.3 MPa, and stirring for 3-8 h to obtain an esterification reaction liquid; (3) cooling the esterification reaction liquid to 20-30 DEG C, separating the solid components in the system by pressure filtration to obtain a filtrate; and (4) sequentially performing normal pressure distillation, vacuum rectification and precision filtration on the filtrate to obtain butyl hafnate. By using the hafnium-based catalyst, the reaction efficiency and product purity of butyl hafnate prepared from hafnium tetrachloride are improved, and the side reaction and equipment corrosion are effectively inhibited. The method has mild process conditions and is suitable for industrial large-scale production of butyl hafnate.

The invention provides a synthesis method of a high-purity hafnium-zirconium metal complex precursor, and belongs to the technical field of high-dielectric-constant materials for super-large-scale integrated circuits. According to the method, hafnium tetrachloride or zirconium tetrachloride is used as a metal source and sequentially reacts with dialkylamine, n-butyllithium and an alkyl magnesium halide Grignard reagent through a one-pot method in a high-purity inert atmosphere, an intermediate does not need to be separated, and a target precursor is obtained after filtration, washing and rectification. The method is simple and convenient in process operation, mild in reaction condition and low in energy consumption; the raw materials are wide in source and low in price, the product yield reaches 82%-88%, and the metal purity is stabilized to be 6N; when the precursor is used for preparing a hafnium oxide / zirconium thin film through atomic layer deposition (ALD), the thickness of the thin film reaches 14.3 nm under 100 cycles, the non-uniformity is smaller than or equal to 0.90%, the requirement of a gate dielectric layer of a super-large-scale integrated circuit for a high-purity and high-efficiency precursor can be met, and the precursor is suitable for industrial amplification production.

The invention belongs to the field of superhigh-temperature ceramic materials, and particularly relates to a hafnium carbide precursor and a preparation method thereof.The preparation method comprises the steps that n-propyl alcohol hafnium and two special modified compounds are mixed in an inert atmosphere, dicumyl peroxide, benzophenone, triethanolamine and divinyl benzene are added for stirring, and the hafnium carbide precursor is obtained; adding tetrahydrofuran, stirring at a constant temperature to form a homogeneous solution, and finally filtering to obtain a precursor; the two modified compounds are vinyl tris (diethylamino) hafnium and acryloyloxy dibenzoyl hafnium complexes respectively, and the preparation method is realized through substitution reaction of hafnium tetrachloride and amine compounds and coordination reaction of n-propanol hafnium, dibenzoylmethane and acryloyl chloride respectively. The obtained hafnium carbide precursor contains a hafnium source, a modified compound, a cross-linking agent and a solvent, through molecular design, the ceramic yield is remarkably increased, the cracking temperature is reduced, the oxidation resistance and sintering density of final ceramic are improved, and the preparation method is suitable for preparing an ultra-high-temperature ceramic material.

This invention discloses a Ru@Zr x Hf y This invention relates to the field of electrocatalysts and its preparation method. The method includes weighing x mmol zirconium tetrachloride, y mmol hafnium tetrachloride, and 1 mmol terephthalic acid, dissolving them in 40–60 mL of DMF to form solution A; adding 3–5 mL of formic acid to solution A to form solution B and then sonicating the solution; subjecting solution B to a hydrothermal reaction to obtain product C; washing and centrifuging product C with a mixed solvent and then drying it under vacuum to obtain powder; dispersing 200 mg of the powder in 30–40 mL of methanol to form solution D; dispersing 0.1–0.3 mmol ruthenium trichloride powder in solution D and stirring to obtain solution E; washing and centrifuging solution E and then drying it under vacuum to obtain a precursor; heating the precursor to 700 °C and holding it for 2–3 h, then cooling it to 300 °C and allowing it to cool naturally to room temperature to obtain Ru@Zr. x Hf y O2 / C electrocatalyst. It solves the problems of high cost of Pt-based catalysts, easy agglomeration and structural damage of traditional Ru-based catalysts, and poor stability due to interference from corrosive ions in seawater electrolysis.

The application discloses a hafnium chloride automatic packaging equipment, which comprises a glove box in which inert gas can be filled, the glove box comprises a transfer cavity and a main cavity, the transfer cavity is an independent cavity body and is arranged at a feeding end of the main cavity; the transfer cavity comprises a vacuum cavity and a plurality of cleaning cavities in sequence along the length direction of the main cavity, and the tail cleaning cavity is communicated with the main cavity. By arranging the independent transfer cavity, the transfer cavity comprises the vacuum cavity and the plurality of cleaning cavities in sequence along the length direction of the main cavity, and is provided with a first air isolation door, a second air isolation door and a vacuumizing assembly, so that a multi-stage material purification buffer zone is jointly constructed. After the material bottle is sent into the transfer cavity through the first conveying element, the material bottle firstly enters the vacuum cavity, the vacuumizing program is started after the second air isolation door is closed, most of the gas and moisture are effectively removed, then the material bottle sequentially passes through the plurality of cleaning cavities, and the circulating purification process of "vacuumizing-inert gas filling" is repeated in each stage cavity, so that the residual oxygen and moisture in the surface and the environment are gradually removed.

The application discloses a purification furnace for tetrachlorohafnium, and relates to the technical field of purification furnaces for tetrachlorohafnium, which comprises a shaft rod installed at the bottom end of the inner cavity of a furnace body through bearings, an impurity accumulation preventing paddle is annularly welded to the outer side of the shaft rod, and a second flow guide ring for annularly dispersing and discharging impurities is welded to the middle part of the inner cavity of the furnace body. The purification furnace for tetrachlorohafnium can timely adjust the reaction conditions in the furnace by dynamically adjusting the opening and closing states of the opening and closing plate, has certain influence on the temperature and pressure in the purification furnace, and can maintain the stability and efficiency of the reaction and purification. The cooperation of the paddle and the opening and closing plate can better separate tetrachlorohafnium gas and impurity particles, a series of flow guide structures facilitate rapid discharge of the impurities in the furnace, reduce the cleaning operation difficulty of workers, buffer the impurities with small particles, prevent a large amount of dust from being generated due to large impact force during discharge, improve the working environment, and protect the health of the operators.

This invention provides a method, apparatus, and semiconductor device for atomic layer etching of hafnium oxide. The method includes performing multiple cycles of etching on the hafnium oxide layer on the top surface of the device to be etched within a reaction chamber until the hafnium oxide layer reaches the target etching requirement. Each cycle includes: adjusting the temperature of the device to be etched to a target reaction temperature; providing a process gas containing a chlorine-based gas; dissociating the process gas into a plasma containing ions and chlorine radicals; filtering the ions in the plasma to obtain chlorine radicals, and reacting the chlorine radicals with the top surface of the hafnium oxide layer at the target reaction temperature to generate a hafnium tetrachloride layer; and heating the device to be etched to a target sublimation temperature to vaporize and discharge the hafnium tetrachloride layer. This invention can reduce the damage to hafnium oxide during etching and achieve higher etching uniformity and precision.

An apparatus includes a body configured to support a substrate, a first coating, conformal on a surface of the body, that is corrosion resistant to at least one of: boron trichloride, nitrogen trifluoride, hafnium tetrachloride, aluminum trichloride, oxygen gas, chlorine gas, fluorine gas, chlorine trifluoride, hydrogen fluoride, hydrogen gas, ammonia, tungsten hexafluoride, tetrafluoromethane, titanium tetrachloride, molybdenum pentachloride, ozone, tetrafluorosilane, or hexafluoroethane, and a second coating, on the first coating, having a hardness that greater than or equal to about 8 gigapascals.

The invention provides a preparation process of hafnium tetrachloride with ultralow niobium content, which comprises the following steps: (1) crushing a hafnium oxide raw material, sieving and drying in vacuum to prepare a pretreated hafnium oxide raw material; (2) preparing a supported composite catalyst; (3) uniformly mixing the pretreated hafnium oxide raw material and a supported composite catalyst according to a mass ratio of (100: 0.5)-(100: 5), and carrying out a chlorination reaction in the presence of chlorine gas at the temperature of 350-500 DEG C and the pressure of 0.1-0.3 MPa to obtain a chlorination reaction product; (4) rectifying and purifying the chlorination reaction product to generate hafnium tetrachloride steam; and (5) condensing the hafnium tetrachloride steam to obtain a hafnium tetrachloride product. The specific supported composite catalyst is adopted, so that the niobium content of the hafnium tetrachloride product is lower than 10 ppb, the purity is larger than or equal to 99.9999%, the preparation efficiency is improved, and the advanced semiconductor manufacturing process requirement can be met.

The application provides a preparation process of hafnium tetrachloride with ultra-low niobium content, comprising the following steps: (1) crushing, sieving and vacuum drying of hafnium oxide raw materials to prepare pretreated hafnium oxide raw materials; (2) preparation of a supported composite catalyst; (3) uniformly mixing the pretreated hafnium oxide raw materials and the supported composite catalyst at a mass ratio of 100:0.5 to 100:5, performing a chlorination reaction in the presence of chlorine at a temperature of 350-500 DEG C and a pressure of 0.1-0.3 MPa to obtain a chlorination reaction product; (4) rectification and purification of the chlorination reaction product to produce hafnium tetrachloride vapor; and (5) condensation of the hafnium tetrachloride vapor to obtain a hafnium tetrachloride product. By using the specific supported composite catalyst, the niobium content of the hafnium tetrachloride product is less than 10 ppb, the purity is greater than or equal to 99.9999%, the preparation efficiency is improved, and the advanced semiconductor process requirements can be met.

The invention belongs to the technical field of membrane separation, and particularly relates to a polydopamine modified metal organic framework material composite membrane, a preparation method and application. The preparation method comprises the following steps: dispersing a polydopamine modified metal organic framework material and polyvinylidene fluoride in a first solvent, and treating by a phase inversion method to obtain a polydopamine modified metal organic framework material composite membrane; the mass ratio of the polydopamine modified metal organic framework material to the polyvinylidene fluoride to the first solvent is (1.8-2.2): (14-16): (80-86); the preparation method of the polydopamine modified metal organic framework material comprises the following steps: dispersing hafnium tetrachloride and 2-aminoterephthalic acid in a first solvent to prepare a metal organic framework material, and dispersing the metal organic framework material and dopamine hydrochloride in a trihydroxymethyl aminomethane hydrochloride buffer solution to obtain the polydopamine modified metal organic framework material. The composite membrane is excellent in piezoelectric catalysis performance and high in pollution resistance and structural stability, water pollutants are efficiently degraded, and the membrane pollution problem is relieved.

This invention relates to the field of dental implant technology, and in particular to a ceramic dental implant, its preparation method, and its application. The preparation method includes the following steps: mixing hafnium tetrachloride and zirconium tetrachloride in benzyl alcohol and reacting to obtain HZO piezoelectric ceramic powder; mixing the HZO piezoelectric ceramic powder with a sintering aid to obtain a mixture; using injection molding to prepare the implant body and abutment separately; sintering the implant body and abutment separately, and assembling them to obtain the ceramic dental implant. This invention, through synergistic optimization of material selection, structural design, interface connection, and surface modification, provides a ceramic dental implant with high safety, excellent mechanical properties, reliable interface connection, and piezoelectric activity, showing promising application prospects.

The application provides a hafnium-based bisphosphonate condensate hydrogel sustained-release system and a preparation method and application thereof, and belongs to the field of bioengineering and material technology. A hafnium tetrachloride solution is added dropwise into a mixed solution containing a bisphosphonate drug and a chemotherapeutic drug, a reaction solution is obtained through liquid-liquid phase separation, and the obtained precipitate is the hafnium-based bisphosphonate condensate hydrogel sustained-release system after stirring and centrifugation. The hafnium-based bisphosphonate condensate hydrogel sustained-release system prepared by the preparation method is disclosed, and the application of the hafnium-based bisphosphonate condensate hydrogel sustained-release system in the preparation of a bone sarcoma radiotherapy sensitization agent and a drug delivery system is disclosed. The hafnium-based bisphosphonate condensate hydrogel sustained-release system prepared by the application has the ideal characteristics of easy preparation, super-high drug loading, pH-dependent controlled release, 'fine tuning' of the release rate, avoidance of drug waste, improvement of the treatment effect and control of adverse side effects.